CN101514981A - Method for rapidly analyzing phase composition of building gypsum powder - Google Patents

Method for rapidly analyzing phase composition of building gypsum powder Download PDF

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Publication number
CN101514981A
CN101514981A CNA2008100579485A CN200810057948A CN101514981A CN 101514981 A CN101514981 A CN 101514981A CN A2008100579485 A CNA2008100579485 A CN A2008100579485A CN 200810057948 A CN200810057948 A CN 200810057948A CN 101514981 A CN101514981 A CN 101514981A
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gypsum
semi
hydrated
percentage composition
dihydrate
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CN101514981B (en
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陈红霞
周梦文
冯菊莲
王霞
颜博渊
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Bnbm Ningbo Co ltd
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Beijing New Building Material Group Co Ltd
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Abstract

The invention provides a method for rapidly analyzing phase composition of building gypsum powder. The method comprises that: step 1, unstable anhydrite III of the building gypsum powder is first transformed into relatively stable semi-hydrated gypsum, and then the content of the anhydrite III is determined according to weight difference before and after transformation; and steps 2, enthalpy values Q1 and Q2 of dihydrate gypsum and the semi-hydrated gypsum in the treated gypsum powder are tested by use of differential scanning calorimetry (DSC), and the content of the dihydrate gypsum and the semi-hydrated gypsum is determined as 100Q1/QDH and 100(Q2/QHH-0.843Q1/QDH) respectively, wherein the QDH and the QHH are the enthalpy values of standard dihydrate gypsum and the semi-hydrated gypsum respectively. The method has the advantages of not only overcoming test errors caused by different gypsum sources or the impurities with crystal water but also greatly shortening the time of three-phase test.

Description

The method of a kind of express-analysis building gypsum plaster phase composition
Technical field
The invention belongs to building material field, specifically is the method for a kind of express-analysis building gypsum plaster phase composition.
Background technology
The phase composition of building gypsum plaster; especially three phase compositions (anhydrite III, semi-hydrated gypsum, dihydrate gypsum) play important effect to the selection and the production quality control of plastering processing parameters such as plasterboard, gypsum block, therefore rapidly and accurately building gypsum plaster are carried out the concern that facies analysis enjoys scale quantity-produced plastering enterprise.
At present, domestic each plastering manufacturing enterprise all operating weight method carries out gypsum three-phase test, promptly utilize dihydrate gypsum, semi-hydrated gypsum under different temperatures dehydration and produce weight difference and calculate and get.Yet the method exists following shortcoming: stipulated in the existing three-phase analytical approach that 1, dihydrate gypsum and semi-hydrated gypsum heat treatment temperature may not all be suitable for all gypsum.Because the temperature that loses water of crystallization of the various places plaster of paris or industry by-product gypsum may be different, therefore may cause institute's test sample product test result bigger than normal or less than normal.2, contain the mineral dehydration of being with water of crystallization in the gypsum and may influence existing method test result.This is particularly evident for the bigger plaster of paris of clay mineral content and purity industry by-product gypsum on the low side.3, the existing method test duration long, this has just weakened the directive function of test result to producing.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of rapid and precise building gypsum plaster facies analysis method, makes the building gypsum plaster facies analysis can instruct the production of plastering manufacturing enterprise immediately and correctly.
In order to address the above problem, the method that the invention provides the phase composition of a kind of express-analysis building gypsum plaster comprises the steps:
Step 1: the unsettled anhydrite III with building gypsum plaster changes into metastable semi-hydrated gypsum earlier, determines the content of anhydrite III according to the weight difference before and after transforming;
Step 2: with dihydrate gypsum and semi-hydrated gypsum heat enthalpy value Q in the above-mentioned treated gesso of differential scanning calorimeter (DSC) test 1And Q 2, the content of determining dihydrate gypsum and semi-hydrated gypsum is for being respectively 100Q 1/ Q DHWith 100 (Q 2/ Q HH-0.843Q 1/ Q DH); Q wherein DHAnd Q HHBe respectively standard dihydrate gypsum and semi-hydrated gypsum heat enthalpy value.
Preferably, described step 1 specifically: taking by weighing weight is W 1Building gypsum plaster, it is tiled in the measuring cup that 55 ℃ of constant weights cross, add 90% ethanolic solution and it flooded powder; Measuring cup is put into 55 ℃ of baking ovens, dry to constant weight, the building gypsum plaster weight after the oven dry is W 2
If W 1<W 2, then the content AIII% of anhydrite III is:
AIII%=15.11×(W 2-W 1)/W 1
If W 1〉=W 2, the content AIII% of anhydrite III is 0.
Preferably, described step 2 is specifically: get an amount of above-mentionedly handle and the building gypsum plaster of oven dry through ethanolic solution, (DSC) tests it with differential scanning calorimeter, experiment condition is as follows: at 0 ℃ of constant temperature, heating rate with 5 ℃/min is warming up to 300 ℃ then, and the rate of temperature fall with 5 ℃/min is cooled to 0 ℃ again; Atmosphere is high-purity N 2, flow 50ml/min; The solid Al of sample disc Du Pont dish;
If W 1〉=W 2, the percentage composition of dihydrate gypsum is 100Q in the sample after then described ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is 100 (Q 2/ Q HH-0.843Q 1/ Q DH); The dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH) (W 2/ W 1);
If W 1<W 2, the percentage composition of dihydrate gypsum is 100Q in the sample after then described ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH), the dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is: 16.11+ (100Q 2/ Q HH-84.3Q 1/ Q DH-16.11) (W 2/ W 1).
The present invention compares with existing building gypsum plaster facies analysis method, has not only overcome the test error that impurity different because of the gypsum source, the band water of crystallization causes, and has shortened three-phase test required time greatly.Therefore, fast construction gesso facies analysis method provided by the invention more helps instant the adjustment and quality control of processing parameter of building product manufacturing enterprise.
Embodiment
Because anhydrite III very easily absorbs airborne moisture, this method has considered that its instability may cause error to the facies analysis result, therefore converts it into metastable semi-hydrated gypsum earlier and tests; Simultaneously, this method has utilized phase transformation heat content and content linear, and the heat content during with differential scanning calorimeter (DSC) test gypsum crystal transition is by calculating the phase composition in the building gypsum plaster;
Concrete steps of the present invention are as follows:
Step 1: (weight is W to take by weighing the building gypsum plaster of about 1g 1), be tiled in the measuring cup that 55 ℃ of constant weights cross, add 90% ethanolic solution and it is flooded powder; Measuring cup is put into 55 ℃ of baking ovens, and drying to constant weight, (weight is W 2);
(1) works as W 1<W 2The time, the content AIII% of anhydrite III is:
AIII%=15.11×(W 2-W 1)/W 1
(2) work as W 1〉=W 2The time, the content AIII% of anhydrite III is 0;
Step 2: get the building gypsum plaster that 10mg handles and dries through ethanolic solution, (DSC) tests it with differential scanning calorimeter.
Experiment condition is as follows: at 0 ℃ of constant temperature, the heating rate with 5 ℃/min is warming up to 300 ℃ then, and the rate of temperature fall with 5 ℃/min is cooled to 0 ℃ again; Atmosphere is high-purity N 2, flow 50ml/min;
(1) standard model test: get pure dihydrate gypsum of analysis and semi-hydrated gypsum sample about 10mg, under above-mentioned test condition, test.2 endothermic peaks are arranged on the DSC curve of dihydrate gypsum, and corresponding respectively dihydrate gypsum is converted into semi-hydrated gypsum, and semi-hydrated gypsum is converted into anhydrite III, and heat content is respectively Q DH, Q HH
(2) building gypsum plaster sample test: get the building gypsum plaster of handling according to step 1 about 10mg, under above-mentioned test condition, test.2 endothermic peaks appear on the DSC curve, corresponding respectively dihydrate gypsum and semi-hydrated gypsum crystal transfer, and heat content is respectively Q 1And Q 2
If in above-mentioned steps 1, work as W 1〉=W 2The time,
The percentage composition of dihydrate gypsum is 100Q in the sample after then ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is 100 (Q 2/ Q HH-0.843Q 1/ Q DH); The dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH) (W 2/ W 1);
If in step 1, work as W 1<W 2The time,
The percentage composition of dihydrate gypsum is 100Q in the sample after then ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH), the dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is: 16.11+ (100Q 2/ Q HH-84.3Q 1/ Q DH-16.11) (W 2/ W 1).
Embodiment 1
Three phase compositions to the building gypsum plaster of desulfurated plaster production are tested with the method that the present invention proposes.Get the building gypsum plaster sample about 1g earlier, pour an amount of 90% ethanolic solution into, and 55 ℃ of baking oven baking constant weights, the content of measuring the anhydrite III in this sample is 16%.The crystal transition heat content of the sample of standard dihydrate gypsum sample and semi-hydrated gypsum is respectively 478.2J/g, 175.1J/g.Under same experimental conditions, be respectively 9.34J/g and 78.62J/g according to obtaining the crystal transition heat content corresponding to the endothermic peak of the crystal transition of dihydrate gypsum and semi-hydrated gypsum on the DSC curve, according to method of the present invention calculate that anhydrite III in the building gypsum plaster is 16%, semi-hydrated gypsum is 72%, dihydrate gypsum is 4.02%.Whole test process obtains test result when shared 4 hours from being sampled to.With traditional three-phase method of testing record in this building gypsum plaster that anhydrite III is 16%, semi-hydrated gypsum is 67.25%, dihydrate gypsum is 7.59%, 8.5 hours whole test process times spent.
Embodiment 2
Three phase compositions to the building gypsum plaster of plaster of paris production are tested with the method that the present invention proposes.Get the building gypsum plaster sample about 1g earlier, pour an amount of 90% ethanolic solution into, and 55 ℃ of baking oven baking constant weights, the content of measuring the anhydrite III in this sample is 25.3%.The crystal transition heat content of the sample of standard dihydrate gypsum sample and semi-hydrated gypsum is respectively 478.2J/g, 175.1J/g.Under same experimental conditions, be respectively 10.01J/g and 51.86J/g according to obtaining the crystal transition heat content corresponding to the endothermic peak of the crystal transition of dihydrate gypsum and semi-hydrated gypsum on the DSC curve, according to method of the present invention calculate that anhydrite III in the building gypsum plaster is 25.3%, semi-hydrated gypsum is 47.5%, dihydrate gypsum is 5.6%.With traditional three-phase method of testing record in this building gypsum plaster that anhydrite III is 25.3%, semi-hydrated gypsum is 40.1%, dihydrate gypsum is 11.2%.This plaster of paris CLAY MINERALS AND THEIR SIGNIFICANCE content is bigger, and when testing with classic method, the water of crystallization in the clay mineral is counted in the dihydrate gypsum, so the measured dihydrate gypsum content value of classic method is bigger than normal.Can avoid causing error to produce with the inventive method, improve test accuracy because of impurity contains water of crystallization.

Claims (3)

1, the method for a kind of express-analysis building gypsum plaster phase composition is characterized in that, comprises the steps:
Step 1: the unsettled anhydrite III with building gypsum plaster changes into metastable semi-hydrated gypsum earlier, determines the content of anhydrite III according to the weight difference before and after transforming;
Step 2: with dihydrate gypsum and semi-hydrated gypsum heat enthalpy value Q in the above-mentioned treated gesso of differential scanning calorimeter (DSC) test 1And Q 2, the content of determining dihydrate gypsum and semi-hydrated gypsum is for being respectively 100Q 1/ Q DHWith 100 (Q 2/ Q HH-0.843Q 1/ Q DH); Q wherein DHAnd Q HHBe respectively standard dihydrate gypsum and semi-hydrated gypsum heat enthalpy value.
2, the method for claim 1 is characterized in that, described step 1 specifically: taking by weighing weight is W 1Building gypsum plaster, it is tiled in the measuring cup that 55 ℃ of constant weights cross, add 90% ethanolic solution and it flooded powder; Measuring cup is put into 55 ℃ of baking ovens, dry to constant weight, the building gypsum plaster weight after the oven dry is W 2
If W 1<W 2, then the content AIII% of anhydrite III is:
AIII%=15.11×(W 2-W 1)/W 1
If W 1〉=W 2, the content AIII% of anhydrite III is 0.
3, method as claimed in claim 1 or 2, it is characterized in that, described step 2 is specifically: get an amount of above-mentionedly handle and the building gypsum plaster of oven dry through ethanolic solution, (DSC) tests it with differential scanning calorimeter, experiment condition is as follows: at 0 ℃ of constant temperature, heating rate with 5 ℃/min is warming up to 300 ℃ then, and the rate of temperature fall with 5 ℃/min is cooled to 0 ℃ again; Atmosphere is high-purity N 2, flow 50ml/min;
If W 1〉=W 2, the percentage composition of dihydrate gypsum is 100Q in the sample after then described ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is 100 (Q 2/ Q HH-0.843Q 1/ Q DH); The dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH) (W 2/ W 1);
If W 1<W 2, the percentage composition of dihydrate gypsum is 100Q in the sample after then described ethanolic solution is handled 1/ Q DH, the percentage composition of semi-hydrated gypsum is (100Q 2/ Q HH-84.3Q 1/ Q DH), the dihydrate gypsum percentage composition is 100 (Q in the primitive architecture gesso 1/ Q DH) (W 2/ W 1), the percentage composition of semi-hydrated gypsum is: 16.11+ (100Q 2/ Q HH-84.3Q 1/ Q DH-16.11) (W 2/ W 1).
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102169073A (en) * 2010-02-25 2011-08-31 北新集团建材股份有限公司 Method for chemically analyzing AII-s phase in building gypsum
CN102175555A (en) * 2011-01-31 2011-09-07 上海市建筑科学研究院(集团)有限公司 Method for quickly analyzing phase component of building gypsum
CN105758761A (en) * 2016-03-01 2016-07-13 美巢集团股份公司 Method for determining content of type III anhydrous gypsum in building gypsum
CN104297096B (en) * 2014-09-26 2016-09-28 西南石油大学 A kind of quantitative determine the method that clay combines water content
CN106323799A (en) * 2015-06-25 2017-01-11 北新集团建材股份有限公司 Method of analyzing crystal water in gypsum plaster boards
CN106814104A (en) * 2015-11-27 2017-06-09 北新集团建材股份有限公司 The method of testing and purposes of ardealite fire resistance
CN111537384A (en) * 2020-04-24 2020-08-14 中铁(天津)隧道工程勘察设计有限公司 Method for determining hydration degree of gypsum rock

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CN100449307C (en) * 2006-06-29 2009-01-07 中电投远达环保工程有限公司 Method for investigating carbonate in gypsum and its device
CN101041439A (en) * 2007-03-01 2007-09-26 武汉理工大学 Method for preparing grammite and sulfuric acid by employing waste slag phosphogypsum

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102169073A (en) * 2010-02-25 2011-08-31 北新集团建材股份有限公司 Method for chemically analyzing AII-s phase in building gypsum
CN102169073B (en) * 2010-02-25 2012-08-29 北新集团建材股份有限公司 Method for chemically analyzing AII-s phase in building gypsum
CN102175555A (en) * 2011-01-31 2011-09-07 上海市建筑科学研究院(集团)有限公司 Method for quickly analyzing phase component of building gypsum
CN102175555B (en) * 2011-01-31 2012-08-22 上海市建筑科学研究院(集团)有限公司 Method for quickly analyzing phase component of building gypsum
CN104297096B (en) * 2014-09-26 2016-09-28 西南石油大学 A kind of quantitative determine the method that clay combines water content
CN106323799A (en) * 2015-06-25 2017-01-11 北新集团建材股份有限公司 Method of analyzing crystal water in gypsum plaster boards
CN106814104A (en) * 2015-11-27 2017-06-09 北新集团建材股份有限公司 The method of testing and purposes of ardealite fire resistance
CN106814104B (en) * 2015-11-27 2020-01-14 北新集团建材股份有限公司 Testing method and application of fire resistance of phosphogypsum
CN105758761A (en) * 2016-03-01 2016-07-13 美巢集团股份公司 Method for determining content of type III anhydrous gypsum in building gypsum
CN105758761B (en) * 2016-03-01 2019-06-11 美巢集团股份公司 The measuring method of type III anhydrous gypsum content in a kind of building gypsum
CN111537384A (en) * 2020-04-24 2020-08-14 中铁(天津)隧道工程勘察设计有限公司 Method for determining hydration degree of gypsum rock
CN111537384B (en) * 2020-04-24 2023-02-03 中铁(天津)隧道工程勘察设计有限公司 Method for determining hydration degree of gypsum rock

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